The present work described two triacontyl-bonded silica adsorbents containing different polar embedded groups (i.e. amide- and carbamate-type) for high performance liquid chromatography, which were prepared by covalent surface modification of silica gel with respective pre-synthesized polar-embedded triacontyl (C30) silane. The acylimidazole-mediated method was used for the first time for the synthesis of amide-type alkyl silane, while the carbamate-type silane was obtained via an improved solvent-free procedure. A conventional C30 stationary phase was also developed on the same silica substrate in the similar manner, which was used as a reference column for comparison of the unique mechanisms facilitated and/or furnished by the polar groups. The successful immobilization of the designed C30 species was confirmed by infrared spectroscopy and elemental analysis. In further comparison with an amide-embedded octadecyl (C18) two other conventional C18 stationary phases of different surface chemistry, detailed chromatographic characterization of the C30 series stationary phases was performed in terms of surface density, hydrophobicity, aromatic selectivity, shape selectivity and water tolerance using a diversified range of analytes, including homologous alkylbenzenes, isomeric polycyclic aromatic hydrocarbons, carotenes, congeners of polychlorobiphenyls, aromatic amines, phenolic compounds, estrogens and nucleosides. A high resemblance between the chromatographic behaviors of the two polar-modified C30 stationary phases was observed, meanwhile they demonstrated noticeable differences from non-polar C30 stationary phase. The polar-embedded C30 phases showed satisfactory performance towards the solutes of interest in the studied conditions. The beneficial synergy of the polar groups and the triacontyl chains enabled these polar-enhanced C30 stationary phases to address challenging separation tasks with high selectivity.

中文翻译：

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液相色谱法设计并评估了含有三aco基的极性嵌入式固定相。

本工作描述了用于高效液相色谱的两种包含不同极性嵌入基团（即酰胺基和氨基甲酸酯型）的三丙烯酰基键合的硅胶吸附剂，这些吸附剂是通过将硅胶分别与预先合成的极性嵌入的三丙烯酰基（ C30）硅烷。酰基咪唑介导的方法首次用于酰胺型烷基硅烷的合成，而氨基甲酸酯型硅烷是通过改进的无溶剂程序获得的。常规的C30固定相也以相似的方式在相同的二氧化硅基质上显影，用作比较极性基团促进和/或提供的独特机理的参考柱。通过红外光谱和元素分析证实了设计的C30物种的成功固定。为了与酰胺嵌入的十八烷基（C18）进行进一步比较，另外两种具有不同表面化学性质的常规C18固定相，根据表面密度，疏水性，芳族选择性，形状选择性和耐水性对C30系列固定相进行了详细的色谱表征使用多种分析物，包括同源的烷基苯，异构的多环芳香烃，胡萝卜素，多氯联苯的同类物，芳香胺，酚类化合物，雌激素和核苷。观察到两个极性修饰的C30固定相的色谱行为非常相似，同时，他们证明了与非极性C30固定相的显着差异。极性嵌入的C30相在研究条件下对感兴趣的溶质表现出令人满意的性能。极性基团和三壬基链的有益协同作用使这些极性增强的C30固定相能够以高选择性解决具有挑战性的分离任务。